反应详情

温度

100 °C

Chloride 12 (23.0 g, 1.0 equiv) was combined with DBU (20.4 g, 2 equiv) in 400 mL xylene and stirred at 100° C. until TLC examination indicated complete reaction (ca. 5 h). The reaction was concentrated to dryness in vacuo. The residue was dissolved in methylene chloride and extracted with water (1×). The organic solvent was removed in vacuo and the residue was flash chromatographed in 10% ethyl acetate/methylene chloride to afford 11.8 g (60%) of 11 as an oil.

1. customreaction (ca. 5 h)
2. concentrationThe reaction was concentrated to dryness in vacuo
3. dissolutionThe residue was dissolved in methylene chloride
4. extractionextracted with water (1×)
5. customThe organic solvent was removed in vacuo
6. customchromatographed in 10% ethyl acetate/methylene chloride